HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 84660332, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 86685926 | HCID 86685926 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 84660332 | HCID 84660332 | 49.3% |
Reaction Steps
To a solution of 1-(6-chloro-7-fluoro-3,4-dihydro-1H-isoquinolin-2-yl)-2,2,2-trifluoroethanone (400 mg) in MeOH (15 mL) was added K2CO3 (572 mg, 4 mmol) in H2O (10 mL). The resulting reaction mixture was stirred at room temperature for 2 hours before it was acidified with HCl (1N) to pH 8. It was then extracted with EtOAc and the organic layer was washed with H2O (2×25 mL), dried over anhy. Na2SO4, filtered and concentrated in vacuo to tive the crude title product together with a regioisomer (170 mg). Prep-TLC separation (30% EtOAc in petroleum ether) then gave the desired title compound (130 mg) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09133158B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-60eb6aff30df4b34a8cbc58ff9431004 |
| Source note | uspto-grants-2015_09 |